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7beta-(t-Butoxycarbonyl)amino-3-[2-(N-tosylcarbamoyl)-benzoyloxy]methyl-3-cephem-4-carboxylic acid → HCID 70582400、化合物

HRID 261717
ノート
印刷プレビュー

反応式

HRID 261717 の反応式
C(OC([NH:8][C@@H:9]1[C:42](=[O:43])[N:11]2[C:12]([C:39]([OH:41])=[O:40])=[C:13]([CH2:16][O:17][C:18](=[O:38])[C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[C:25](=[O:37])[NH:26][S:27]([C:30]3[CH:36]=[CH:35][C:33]([CH3:34])=[CH:32][CH:31]=3)(=[O:29])=[O:28])[CH2:14][S:15][C@H:10]12)=O)(C)(C)C>FC(F)(F)C(O)=O>[NH2:8][C@@H:9]1[C:42](=[O:43])[N:11]2[C:12]([C:39]([OH:41])=[O:40])=[C:13]([CH2:16][O:17][C:18](=[O:38])[C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][C:20]=3[C:25](=[O:37])[NH:26][S:27]([C:30]3[CH:36]=[CH:35][C:33]([CH3:34])=[CH:32][CH:31]=3)(=[O:29])=[O:28])[CH2:14][S:15][C@H:10]12
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 705836227beta-(t-Butoxycarbonyl)amino-3-[2-(N-tosylcarbamoyl)-benzoyloxy]methyl-3-cephem-4-carboxylic acid

生成物 1

HCID 70582400HCID 70582400、化合物収率 90.4%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

7β-(t-Butoxycarbonyl)amino-3-[2-(N-tosylcarbamoyl)benzoyloxy]methyl-3-cephem-4-carboxylic acid (631 mg) is dissolved in trifluoroacetic acid (2 ml) under ice-cooling. The solution is stirred for 20 minutes and concentrated under reduced pressure. To the residue, ether (20 ml) is added and the resultant solid is triturated. The powder thus obtained is collected by filtration, washed with ether and dried over phosphorus pentoxide. The procedure provides 7β-amino-3-[2-(N-tosylcarbamoyl)benzoyloxy]methyl-3-cephem-4-carboxylic acid (480 mg).

後処理

  1. temperaturecooling
  2. concentrationconcentrated under reduced pressure
  3. additionTo the residue, ether (20 ml) is added
  4. customthe resultant solid is triturated
  5. customThe powder thus obtained
  6. filtrationis collected by filtration
  7. washwashed with ether
  8. dry with materialdried over phosphorus pentoxide

出典と根拠

ORDレコード
ord-44d669d78396485f9e0c74dd0aea5711
出典データセット
uspto-grants-1979_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04166178

反応ノート

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